CN103774096A - Preparation method for anti-oxidation composite hard coating - Google Patents
Preparation method for anti-oxidation composite hard coating Download PDFInfo
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- CN103774096A CN103774096A CN201310576458.7A CN201310576458A CN103774096A CN 103774096 A CN103774096 A CN 103774096A CN 201310576458 A CN201310576458 A CN 201310576458A CN 103774096 A CN103774096 A CN 103774096A
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- 238000000576 coating method Methods 0.000 title claims abstract description 108
- 239000011248 coating agent Substances 0.000 title claims abstract description 106
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 230000003064 anti-oxidating effect Effects 0.000 title abstract 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 37
- 230000007704 transition Effects 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000004544 sputter deposition Methods 0.000 claims abstract description 7
- 238000007733 ion plating Methods 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 3
- 230000008020 evaporation Effects 0.000 claims abstract description 3
- 239000010936 titanium Substances 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 230000003078 antioxidant effect Effects 0.000 claims description 13
- 239000003963 antioxidant agent Substances 0.000 claims description 12
- 235000006708 antioxidants Nutrition 0.000 claims description 12
- 238000005266 casting Methods 0.000 claims description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 239000000956 alloy Substances 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 6
- 238000005488 sandblasting Methods 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- UZQSJWBBQOJUOT-UHFFFAOYSA-N alumane;lanthanum Chemical compound [AlH3].[La] UZQSJWBBQOJUOT-UHFFFAOYSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000005238 degreasing Methods 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 15
- 229910010037 TiAlN Inorganic materials 0.000 abstract description 11
- 238000012360 testing method Methods 0.000 abstract description 8
- 238000005520 cutting process Methods 0.000 abstract description 4
- 238000007373 indentation Methods 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract 2
- 238000007254 oxidation reaction Methods 0.000 abstract 2
- 239000002004 ayurvedic oil Substances 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 238000003825 pressing Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 230000002045 lasting effect Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 229910000997 High-speed steel Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 238000010301 surface-oxidation reaction Methods 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- -1 can see Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- Cutting Tools, Boring Holders, And Turrets (AREA)
- Physical Vapour Deposition (AREA)
Abstract
本发明公开了一种切削刀具表面抗氧化复合硬质涂层的制备方法，包括工件加热、工件等离子体清洗、过渡层制备、涂层制备、冷却步骤，以坩埚内的Ti铸锭作为TiN过渡层的Ti源，通过热阴极离子镀中的柱弧电源电流控制Ti铸锭的蒸发速度；以平面TiAlLa靶作为（TiAlLa）N涂层对应元素的来源，通过调节中频脉冲电源的功率控制靶材的溅射率；采用高纯Ar作为离化气体。采用N2作为反应气体。该方法制备的（TAlLa）N涂层厚度约为2微米，纳米硬度40Gpa以上，抗氧化温度可以达到900℃以上，压痕实验等级为HF1(德国标准VDI3198)，与TiAlN涂层相比，具有更好的抗氧化性和机械性能，使用寿命更长。
The invention discloses a method for preparing an anti-oxidation composite hard coating on the surface of a cutting tool, which includes the steps of workpiece heating, workpiece plasma cleaning, transition layer preparation, coating preparation, and cooling steps. Ti ingot in a crucible is used as TiN transition The Ti source of the layer, the evaporation rate of the Ti ingot is controlled by the column arc power supply current in the hot cathode ion plating; the planar TiAlLa target is used as the source of the corresponding elements of the (TiAlLa)N coating, and the target is controlled by adjusting the power of the intermediate frequency pulse power supply The sputtering rate; using high-purity Ar as the ionization gas. N2 was employed as the reactive gas. The thickness of the (TAILa)N coating prepared by this method is about 2 microns, the nanohardness is above 40Gpa, the oxidation resistance temperature can reach above 900°C, and the indentation test level is HF1 (German standard VDI3198). Compared with TiAlN coating, it has Better oxidation resistance and mechanical properties, longer service life.
Description
Technical field
The present invention relates to a kind of preparation method of cutting tool surface oxidation-resistant coating material, relate in particular to a kind of preparation method of cutting tool surface oxidation-resistant composite hard coating material.
Background technology
Along with the development of processing technology, tooling cost is also in continuous progress.Cutter coat can improve hardness, wear resistance and the oxidation-resistance of tool surface effectively, thereby can allow cutter tackle harsher machining condition simultaneously the work-ing life of having improved to a certain extent cutter.The cutter coat of application is TiN coating the earliest, and its wear resistance and oxidation-resistance improve a lot compared with tool matrix.Afterwards on the basis of TiN again development the coating such as TiAlN, TiAlCrN and TiAlSiN, these coatings improve in hardness and wear resistance, but oxidation-resistance be still difficult to meet day by day improve machining condition.
Summary of the invention
The problem of the oxidation-resistance deficiency based on traditional hard coat performance, the invention provides the preparation method of a kind of oxidation-resistance rigid composite coating TiN/ (TiAlLa) N that has added earth La.First preparing one deck TiN transition layer at workpiece surface by hot cathode ion plating makes coating entirety have more excellent comprehensive mechanical property; Use TiAlLa composite alloy target to be more conducive to control the stability of technique.
A preparation method for anti-oxidant rigid composite coating, comprises workpiece heating, workpiece plasma clean, transition layer preparation, coating preparation process,
1) the Ti source of described transition layer preparation using the Ti ingot casting in crucible as TiN transition layer, by the velocity of evaporation of the post arc power current control Ti ingot casting in hot cathode ion plating;
2) described coating is prepared the source using plane TiAlLa target as (TiAlLa) N coating corresponding element, by regulating the sputtering raste of power control target of medium-frequency pulse power supply;
3) adopt high-purity Ar as ionization of gas.Guarantee effective glow discharging process.
4) adopt N
2as reactant gases, make its ionization and be combined with Ti, Al, La element, in matrix surface formation of deposits (TiAlLa) N coating.
Compound coating has lower frictional coefficient and wear rate compared with single coating, therefore TiN/ (TiAlLa) N compound coating energy
The better shortcoming that solves coating oxidation-resistance deficiency.
Described preparation method first will put into after substrate pretreated on the fixture of hot cathode ion plating and medium frequency magnetron sputtering composite coating equipment, and this fixture rotates with pivoted frame platform, rotation simultaneously.To guarantee the homogeneity of coating process.
At described workpiece heating steps, workpiece packs into after coating chamber, first coating chamber is evacuated to 5.0 × 10
-3pa, then passes into Ar, and controlling total pressure in coating chamber is 3.0 × 10
-1～4.5 × 10
-1pa, opens hot-cathode, and post arc current is 140～180A, to workpiece heating 40～150min.
In workpiece plasma clean step, regulate Ar flow, make coating chamber internal gas pressure remain on 1.5 × 10
-1～2.0 × 10
-1pa, post arc current is 110～160A, workpiece direct current (DC) bias-100～200V, pulsed bias-400～-800V, with the plasma body of 7.0～10.0KW to workpiece surface Bombardment and cleaning, time length 15～50min;
In transition layer preparation process, after workpiece cleaning completes, regulate Ar flow, and pass into N in coating chamber
2, Ar/N
2remain on 1/1.5～1/3, in coating chamber, pressure is 3.0 × 10
-1～4.5 × 10
-1pa, post arc current is 180～220A, workpiece direct current (DC) bias-100～200V, pulsed bias-400～-800V, is coated with one deck TiN transition layer at workpiece surface with the hot-cathode ion of power 11.0～14.0KW, is coated with time 5～20min.
In coating preparation process, direct current (DC) bias is adjusted into-40～-70V, by Ar/N
2be 1/1.5～1/3 in coating chamber, to pass into Ar and N
2mixed gas, regulating pressure in coating chamber is 3.0 × 10
-1～4.5 × 10
-1pa, post arc current remains on 100～110A, opens the control power supply of TiAlLa target, and target power supply electric current remains on 4.0～7.0A, on TiN transition layer, carry out (TiAlLa) N coating with the medium frequency magnetron sputtering of power 3.0～5.0KW and prepare, be coated with time 120～240min.
Described pre-treatment comprises surface degreasing, immerses ultrasonic cleaning and oven dry in alcohol after sandblasting.
Described TiAlLa target is TixAl
yla
l-x-Ycomposite alloy target, its titanium aluminium lanthanum atomic ratio is 60～70: 20～40: 1～5, purity is 99.99%.
Cooling 60～150min after the preparation of described (TiAlLa) N coating.
Totally four of described plane TiAlLa targets, and be placed in mode facing each other on the inwall of coating chamber.
After measured, TiN/ (TiAlLa) N rigid composite coating prepared by the inventive method, thickness is 2 microns.
Adopt nanohardness tester (MTS Systems Corp., Oak Ridge, TN, USA) test, more than nano hardness 40Gpa.Through contrast experiment, TiN/TiAlLaN coating has higher consistency and elasticity modulus compared with TiAlN coating, has better wear resistance, longer service life.
Adopt Rockwell pressing in method (HR-150A Rockwell hardness instrument) test, TiN/TiAlLaN coating indentation test grade is HFl, has mechanical property.Through contrast experiment, TiN/TiAlLaN coating is finer and closely woven than TiAlN coating (impression grade is HF3) tissue, and purity is higher, surfacing.Bonding force is better, incrust, and consistence and the homogeneity of thickness are better.Be particularly suitable for applying on high-speed dry type cutting cutter.
Prepared TiN/ (TiAlLa) N rigid composite coating is heated to 900 ℃ in air, be incubated 2 hours, after cool to room temperature, adopt XRD Xing to penetrate instrument (PW-1700 type, Philips) detect its oxide content well below general T iAlN coating through XRD, show that coating has good antioxidant property.
Accompanying drawing explanation
Fig. 1 is the fracture schematic diagram of TiAlN coating.
Fig. 2 is the fracture schematic diagram of TiN/ (TiAlLa) N rigid composite coating.
Fig. 3 is the bonding force schematic diagram of TiAlN coating.
Fig. 4 is the bonding force schematic diagram of TiN/ (TiAlLa) N rigid composite coating.
Fig. 5 is that TiN/ (TiAlLa) N rigid composite coating and general T iAlN are heated to 900 ℃ and be incubated XRD figure after 2 hours spectrum in air.
Embodiment
Embodiment below in conjunction with embodiment is described in further detail foregoing of the present invention again.But this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following examples.Without departing from the idea case in the present invention described above, various replacements or the change made according to ordinary skill knowledge and customary means, all should be included in protection scope of the present invention.
Embodiment 1
By ordinary method, carbide-tipped milling cutter is carried out putting into coating chamber after oil removing, sandblasting and ultrasonic cleaning, then coating chamber is evacuated to 5.0 × 10
-3pa, passes into argon gas, and making total pressure in vacuum chamber is 4.0 × 10
-1pa, and to control post arc current be that 150A treats and is coated with cutter heating 150min; At pressure 1.8 × 10
-1under the argon shield of Pa, control the direct current (DC) bias of cutter and be-200V, pulsed bias-600V, controlling post arc current is 120A, cutter is waited to cleaning, lasting 30min with the plasma body of 7.0KW; Pass into Ar/N
2=1/2 Ar and N
2mixed gas, keep pressure be 3.0 × 10
-1pa, with post arc heating Ti ingot casting, post arc current is 180A, power is 11.0KW, at direct current (DC) bias-200V, under pulsed bias-400V, is coated with 10min; Keep Ar/N
2=i/2 and 3.0 × 10
-1the pressure of Pa, use medium frequency magnetron sputtering sputtered with Ti: Al: La=69: the composite alloy target of 30: 1, sputtering current is 5.0A, power is 3.0KW, under direct current (DC) bias-50V, is coated with 150min; Naturally cooling 90min, takes out cutter.
On this carbide-tipped milling cutter, apply after TiN/ (TiAlLa) N rigid composite coating, adopt nanohardness tester (MTSSystems Corp., Oak Ridge, TN, USA) recording hardness is 41～44Gpa, and coat-thickness is 2 microns, TiN transition region thickness 200 nanometers, adopt Rockwell pressing in method (HR-150A Rockwell hardness instrument) test, impression grade is HFl.
Prepared TiN/ (TiAlLa) N rigid composite coating is heated to 900 ℃ in air, be incubated 2 hours, after cool to room temperature, adopt XRD Xing to penetrate instrument (PW-1700 type, Philips) detect and still retain coated component through XRD, show that coating has good oxidation-resistance.
Embodiment 2
By ordinary method, carbide-tipped lathe tool is carried out putting into coating chamber after oil removing, sandblasting and ultrasonic cleaning, then coating chamber is evacuated to 5.0 × 10
-3(claim is 5.0 × 10 to pa
-3pa), pass into argon gas, making total pressure in vacuum chamber is 4.0 × 10
-1pa, and to control post arc current be that 160A treats and is coated with cutter heating 80min; At pressure 1.5 × 10
-1under the argon shield of Pa, control the direct current (DC) bias of cutter and be-200V, pulsed bias-500V, controlling post arc current is 130A, cutter is waited to cleaning, lasting 30min with the plasma body of 8.0KW; Pass into Ar/N
2=1/3 Ar and N
2mixed gas, keep pressure be 3.5 × 10
-1pa, with post arc heating Ti ingot casting, post arc current is 200A, power is 12.0KW, at direct current (DC) bias-200V, under pulsed bias-500V, is coated with 10min; Keep Ar/N
2=1/3 and 3.5 × 10
-1the pressure of pa, use medium frequency magnetron sputtering sputtered with Ti: Al: La=69: the composite alloy target of 29: 2, sputtering current is 7.0A, power is 4.0KW, under direct current (DC) bias-45V, is coated with 200min; Naturally cooling 90min, takes out cutter.
On this carbide-tipped lathe tool, apply after TiN/ (TiAlLa) N rigid composite coating, adopt nanohardness tester (MTSSystems Corp., Oak Ridge, TN, USA) recording hardness is 43～45Gpa, and coat-thickness is 2 microns, TiN transition region thickness 200 nanometers, adopt Rockwell pressing in method (HR-150A Rockwell hardness instrument) test, impression grade is HFl.
Prepared TiN/ (TiAlLa) N rigid composite coating is heated to 900 ℃ in air, be incubated 2 hours, after cool to room temperature, adopt XRD Xing to penetrate instrument (PW-1700 type, Philips) detect and still retain coated component through XRD, show that coating has good oxidation-resistance.
Embodiment 3
By ordinary method, high speed steel screw tap is carried out putting into coating chamber after oil removing, sandblasting and ultrasonic cleaning, then coating chamber is evacuated to 5.0 × 10
-3pa, passes into argon gas, and making total pressure in vacuum chamber is 3.0 × 10
-1pa, and to control post arc current be that 140A treats and is coated with cutter heating 40min; At pressure 1.5 × 10
-1under the argon shield of pa, control the direct current (DC) bias of cutter and be-100V, pulsed bias-500V, controlling post arc current is 140A, cutter is cleaned with the plasma body of 9.0KW lasting 15min; Pass into Ar/N
2=1/1.5 Ar and N
2mixed gas, keep pressure be 3.0 × 10
-1pa, with post arc heating Ti ingot casting, post arc current is 180A, power is 13.0KW, at direct current (DC) bias-100V, under pulsed bias-500V, is coated with 5min; Keep Ar/N
2=1/1.5 and 3.0 × 10
-1the pressure of Pa, use medium frequency magnetron sputtering sputtered with Ti: Al: La=69: the composite alloy target of 30: 1, sputtering current is 4.0A, power is 3.5KW, under direct current (DC) bias-40V, is coated with 120min; Naturally cooling 60min, takes out cutter.
On this high speed steel screw tap, apply after TiN/ (TiAlLa) N rigid composite coating, adopt nanohardness tester (MTS Systems Corp., Oak Ridge, TN, USA) recording hardness is 39～41Gpa, and coat-thickness is 2 microns, TiN transition region thickness 200 nanometers, adopt Rockwell pressing in method (HR-150A Rockwell hardness instrument) test, impression grade is HF1.
Prepared TiN/ (TiAlLa) N rigid composite coating is heated to 900 ℃ in air, is incubated 2 hours, after cool to room temperature, adopt XRD Xing to penetrate instrument (PW
-1700 types, Philips) detect and still retain coated component through XRD, show that coating has good oxidation-resistance.
Embodiment 4
By ordinary method, carbide hob is carried out putting into coating chamber after oil removing, sandblasting and ultrasonic cleaning, then coating chamber is evacuated to 5.0 × 10
-3pa, passes into argon gas, and making total pressure in vacuum chamber is 4.5 × 10
-1pa, and to control post arc current be that 180A treats and is coated with cutter heating 100min; At pressure 2.0 × 10
-1under the argon shield of Pa, control the direct current (DC) bias of cutter and be-200V, pulsed bias-800V, controlling post arc current is 160A, cutter is cleaned with the plasma body of 10.0KW lasting 50min; Pass into Ar/N
2=1/3 Ar and N
2mixed gas, keep pressure be 4.5 × 10
-1pa, with post arc heating Ti ingot casting, post arc current is 220A, power is 14.0KW, at direct current (DC) bias-200V, under pulsed bias-800V, is coated with 20min; Keep Ar/N
2=1/3 and 4.5 × 10
-1the pressure of Pa, use medium frequency magnetron sputtering sputtered with Ti: Al: La=67: the composite alloy target of 28: 5, sputtering current is 7.0A, power is 5.0KW, under direct current (DC) bias-70V, is coated with 240min; Naturally cooling 150min, takes out cutter.
This carbide hob applies after TiN/ (TiAlLa) N rigid composite coating, adopt nanohardness tester (MTS Systems Corp., Oak Ridge, TN, USA) recording hardness is 41～43Gpa, and coat-thickness is 2 microns, TiN transition region thickness 200 nanometers, adopt Rockwell pressing in method (HR-150A Rockwell hardness instrument) test, impression grade is HFl.
Prepared TiN/ (TiAlLa) N rigid composite coating is heated to 900 ℃ in air, is incubated 2 hours, after cool to room temperature, adopt XRD Xing to penetrate instrument (PW-1700 type, Philips) and detect and still retain coated component through XRD, table
Bright coating has good oxidation-resistance.
| ? | Cooling time |
| Claims | 60～150min |
| Embodiment 1 | 90min |
| Embodiment 2 | 90min |
| Embodiment 3 | 60min |
| Embodiment 4 | 150min |
Contrast experiment:
1. hardness contrast
Adopt nanohardness tester (MTS Systems Corp., Oak Ridge, TN, USA), the hardness of contrast TiAlNTiN/TiAlLaN coating, can see, TiN/TiAlLaN coating has higher hardness and lower Young's modulus compared with TiAlN.
2. fracture contrast
Adopt scanning electron microscope (S300-N, Hitachi, Japan), observe and obtain Fig. 1,2.TiAlN coating in accompanying drawing 1 has more obvious column crystal form, and the crystal habit of TiN/TiAlLaN coating in accompanying drawing 2 is more tiny, fine and close.
3. bonding force contrast
Adopt Rockwell pressing in method (HR-150A Rockwell hardness instrument), observe and obtain accompanying drawing 3,4.TiAlN coating in accompanying drawing 3, impression grade is HF3, the TiN/TiAlLaN coating in accompanying drawing 4, impression grade is HFl, and peeling off of visible TiAlN coating is more serious, and bonding force is poorer.
4. oxidation-resistance contrast
In air, be heated to 900 ℃, be incubated 2 hours, after cool to room temperature, adopt XRD Xing to penetrate instrument (PW-1700 type, Philips) carry out XRD detection, find that TiN/TiAlLaN coating still retains coated component (accompanying drawing 5), have obvious TiN Xing to penetrate peak, show that coating has good oxidation-resistance.TiAlN coating under the same terms is all oxidized, and has SiO, TiO
2, γ-A1
2o
3.
Claims (10)
1. a preparation method for anti-oxidant rigid composite coating, comprises workpiece heating, workpiece plasma clean, transition layer preparation, coating preparation, cooling step, it is characterized in that:
1) the Ti source of described transition layer preparation using the Ti ingot casting in crucible as TiN transition layer, by the velocity of evaporation of the post arc power current control Ti ingot casting in hot cathode ion plating;
2) described coating is prepared the source using plane TiAlLa target as (Ti, Al, La) N coating corresponding element, by regulating the sputtering raste of power control target of medium-frequency pulse power supply;
3) adopt high-purity Ar as ionization of gas;
4) adopt N
2as reactant gases, make its ionization and be combined with Ti, Al and La element, in matrix surface formation of deposits (TiAlLa) N coating.
2. the preparation method of a kind of anti-oxidant rigid composite coating as claimed in claim 1, it is characterized in that: first will after substrate pretreated, put on the fixture of hot cathode ion plating and medium frequency magnetron sputtering composite coating equipment, this fixture rotates with pivoted frame platform, rotation simultaneously.
3. the preparation method of a kind of anti-oxidant rigid composite coating as claimed in claim 1 or 2, is characterized in that: at described workpiece heating steps, workpiece packs into after coating chamber, first coating chamber is evacuated to 5.0 × 10
-3pa, then passes into Ar, and controlling total pressure in coating chamber is 3.0 × 10
-1～4.5 × 10
-1pa, opens hot-cathode, and post arc current is 140～180A, to workpiece heating 40～150min.
4. the preparation method of a kind of anti-oxidant rigid composite coating as claimed in claim 1 or 2, is characterized in that: in workpiece plasma clean step, regulate Ar flow, make coating chamber internal gas pressure remain on 1.5 × 10
-1～2.0 × 10
-1pa, post arc current is 110～160A, workpiece direct current (DC) bias-100～-200V, pulsed bias-400～-800V, with the plasma body of 7.0～10.0KW to workpiece surface Bombardment and cleaning, time length 15～50min.
5. the preparation method of a kind of anti-oxidant rigid composite coating as claimed in claim 1 or 2, is characterized in that: in transition layer preparation process, after workpiece cleaning completes, regulate Ar flow, and pass into N in coating chamber
2, Ar/N
2remain on 1/1.5～1/3, in coating chamber, pressure is 3.0 × 10
-1～4.5 × 10
-1pa, post arc current is 180～220A, workpiece direct current (DC) bias-100～-200V, pulsed bias-400～-800V, is coated with one deck TiN transition layer at workpiece surface with the hot-cathode ion of power 11.0～14.0KW, is coated with time 5～20min.
6. the preparation method of a kind of anti-oxidant rigid composite coating as claimed in claim 1 or 2, is characterized in that: in coating preparation process, direct current (DC) bias is adjusted into-40～-70V, by Ar/N
2be 1/1.5～1/3 in coating chamber, to pass into Ar and N
2mixed gas, regulating pressure in coating chamber is 3.0 × 10
-1～4.5 × 10
-1pa, post arc current remains on 100～110A, opens the control power supply of TiAlLa target, and target power supply electric current remains on 4.0～7.0A, on TiN transition layer, carry out (TiAlLa) N coating with the medium frequency magnetron sputtering of power 3.0～5.0KW and prepare, be coated with time 120～240min.
7. the preparation method of a kind of anti-oxidant rigid composite coating as claimed in claim 2, is characterized in that: described pre-treatment comprises surface degreasing, immerses ultrasonic cleaning and oven dry in alcohol after sandblasting.
8. the preparation method of a kind of anti-oxidant rigid composite coating as claimed in claim 1, is characterized in that: described TiAlLa target is Ti
xal
yla
1-X-Ycomposite alloy target, its titanium aluminium lanthanum atomic ratio is 60～70:20～40:1～5, purity is 99.99%.
9. the preparation method of a kind of anti-oxidant rigid composite coating as claimed in claim 1, is characterized in that: (TiAlLa) cooling 60～150min after the preparation of N coating.
10. the preparation method of a kind of anti-oxidant rigid composite coating as claimed in claim 1, is characterized in that: totally four of described plane TiAlLa targets, and be placed in mode facing each other on the inwall of coating chamber.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104789933A (en) * | 2015-04-28 | 2015-07-22 | 重庆文理学院 | Nano composite coating and deposition method thereof |
| CN104862652A (en) * | 2015-05-11 | 2015-08-26 | 上海应用技术学院 | Method for manufacturing TiAlSiN super-hard gradient coating |
| CN107130213A (en) * | 2017-05-03 | 2017-09-05 | 成都真锐科技涂层技术有限公司 | Multicomponent alloy laminated film Preparation equipment and preparation method |
| RU2641438C1 (en) * | 2017-03-10 | 2018-01-17 | федеральное государственное бюджетное образовательное учреждение высшего образования "Ульяновский государственный технический университет" | Method for production of multilayer coating for cutting tool |
| CN113667931A (en) * | 2021-08-19 | 2021-11-19 | 嘉兴鸷锐新材料科技有限公司 | Lanthanide rare earth oxide composite TiSiN coating |
| CN113943929A (en) * | 2021-10-18 | 2022-01-18 | 河南科技大学 | A kind of preparation method of TiLaN composite film and wear-resistant product |
| CN114941126A (en) * | 2022-06-29 | 2022-08-26 | 武汉苏泊尔炊具有限公司 | Antibacterial cutter and manufacturing method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104789933A (en) * | 2015-04-28 | 2015-07-22 | 重庆文理学院 | Nano composite coating and deposition method thereof |
| CN104789933B (en) * | 2015-04-28 | 2017-06-20 | 重庆文理学院 | A kind of nano-composite coating and its deposition process |
| CN104862652A (en) * | 2015-05-11 | 2015-08-26 | 上海应用技术学院 | Method for manufacturing TiAlSiN super-hard gradient coating |
| RU2641438C1 (en) * | 2017-03-10 | 2018-01-17 | федеральное государственное бюджетное образовательное учреждение высшего образования "Ульяновский государственный технический университет" | Method for production of multilayer coating for cutting tool |
| CN107130213A (en) * | 2017-05-03 | 2017-09-05 | 成都真锐科技涂层技术有限公司 | Multicomponent alloy laminated film Preparation equipment and preparation method |
| CN107130213B (en) * | 2017-05-03 | 2019-04-09 | 成都真锐科技涂层技术有限公司 | Multi-component alloy composite film preparation equipment and preparation method |
| CN113667931A (en) * | 2021-08-19 | 2021-11-19 | 嘉兴鸷锐新材料科技有限公司 | Lanthanide rare earth oxide composite TiSiN coating |
| CN113943929A (en) * | 2021-10-18 | 2022-01-18 | 河南科技大学 | A kind of preparation method of TiLaN composite film and wear-resistant product |
| CN114941126A (en) * | 2022-06-29 | 2022-08-26 | 武汉苏泊尔炊具有限公司 | Antibacterial cutter and manufacturing method thereof |
| CN114941126B (en) * | 2022-06-29 | 2023-08-25 | 武汉苏泊尔炊具有限公司 | Antibacterial cutter and manufacturing method thereof |
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